Method for detecting contents of potassium oxide and sodium oxide in blast furnace ash

Through high-temperature burning and atomic absorption spectroscopy measurement methods, the problem of potassium oxide and sodium oxide detection in blast furnace ash was solved, and accurate and economical detection effects were achieved, providing technical support for the safety and anterior direction of blast furnace.

CN120195119APending Publication Date: 2025-06-24BENGANG STEEL PLATES CO LTD
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Patent Information

Application Number
CN202510491248.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-18
Publication Date
2025-06-24

AI Technical Summary

Technical Problem

The prior art is difficult to effectively detect the content of potassium oxide and sodium oxide in blast furnace ash, which affects the safety and anterior direction of blast furnace.

Method used

A method including high-temperature calcination, heating digestion and atomic absorption spectroscopy is used to measure the content of potassium and sodium by weighing blast furnace ash samples, and the mass content of their oxides is calculated after digestion.

Benefits of technology

It realizes accurate detection of the potassium oxide and sodium oxide content in blast furnace ash, which is low in cost and simple in steps. It is suitable for most laboratories and provides technical support for blast furnace directedness.

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Abstract

The invention relates to the technical field of analytical chemistry, in particular to a method for detecting the content of potassium oxide and sodium oxide in blast furnace ash, which comprises the following steps: weighing 0.1-0.5 g of blast furnace ash sample for production, burning at high temperature, removing free carbon completely, and cooling to room temperature; adding water to wet the sample, adding 7-20 mL of concentrated hydrochloric acid, 5-10 mL of hydrofluoric acid and 5-10 mL of perchloric acid, heating at 260-290 DEG C until perchloric acid smoke is emitted, and continuously heating and evaporating until the perchloric acid smoke is nearly dry; adding 10-20mL of hydrochloric acid, heating to dissolve salts, transferring the solution into a plastic volumetric flask, cooling to room temperature, diluting with water to a set scale, and uniformly mixing to obtain a potassium and sodium standard solution; diluting the potassium standard solution and the sodium standard solution step by step to obtain a calibration curve, measuring the calibration curve and the solution to be measured by using an atomic absorption spectrometer, and calculating the mass contents of potassium oxide and sodium oxide in the blast furnace ash; the method is low in cost, simple in steps and easy to operate, and the content of potassium oxide and sodium oxide in the blast furnace ash can be detected.
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Description

Technical Field

[0001] The present invention relates to the technical field of analytical chemistry, and particularly to a method for detecting the contents of potassium oxide and sodium oxide in blast furnace ash. Background Art

[0002] In iron and steel production, potassium, sodium and their oxides will deposit and enter the brick joints of the blast furnace. If not controlled in time, the deposits will cause the furnace wall and pipes to thicken, affecting the safety of the hearth and the blast furnace and the smooth operation of the blast furnace. Blast furnace ash is one of the raw materials charged into the blast furnace and is widely used. There are many types of raw materials charged into the blast furnace, and the batching is complex. These raw materials contain different contents of potassium, sodium and their oxides. For the safety of the blast furnace, it is necessary to regularly detect the potassium and sodium contents in the raw materials charged into the blast furnace, and based on the detection results, adjust and control the batching in time to ensure the smooth operation of the blast furnace.

[0003] Chinese Patent with Publication No. CN116178788B discloses a method for preparing a hydrotalcite-type nano flame retardant using blast furnace ash and chromium-containing aluminum mud. By mixing blast furnace ash and chromium-containing aluminum mud and performing reduction roasting, the iron oxides in the blast furnace ash and the chromium oxides in the chromium-containing aluminum mud are reduced to form ferrochromium alloy. Then, through crushing and grinding, the monomer dissociation of the ferrochromium alloy is achieved. Then, through magnetic separation, the magnetic product ferrochromium alloy and the non-magnetic product high-aluminum slag (mainly containing alumina) are separated. Then, in a CO2 atmosphere, the high-aluminum slag, magnesium-containing reagent and water are subjected to mechanochemical reaction. Under the mechanochemical action, the alumina in the high-aluminum slag and the magnesium in the magnesium-containing reagent react with water and carbon dioxide to form a nano flame retardant containing magnesium-aluminum carbonate-type hydrotalcite; however, this application is not applicable to the detection of potassium oxide and sodium oxide in blast furnace ash.

[0004] The paper "Determination of Zinc in Blast Furnace Ash by Inductively Coupled Plasma Atomic Emission Spectrometry" has important guiding significance for the scientific reuse of blast furnace ash by accurately determining the zinc content in blast furnace ash. The components of blast furnace ash are complex, containing ore, refractory materials, coal coke, etc. The sample pretreatment process is complex and the detection is difficult. Using hydrochloric acid-nitric acid-hydrofluoric acid-hydrogen peroxide as the digestion system and treating the sample by microwave digestion method, complete digestion of the sample is achieved. Selecting Zn206.201nm as the analysis line, the sample solution is determined by inductively coupled plasma atomic emission spectrometry (ICP-AES), and a method for determining zinc in blast furnace ash is established. Under the optimized experimental conditions, the mass concentration of zinc has a linear relationship with its corresponding emission intensity in the range of 5.00 - 100.00 μg / mL, and the linear correlation coefficient is 0.9999. The detection limit of the method is 0.00092% (mass fraction). The matrix effect is investigated, and the results show that the iron matrix in blast furnace ash has no significant influence on the determination of zinc. According to the experimental method, the relative standard deviation (RSD, n = 11) of the results for determining zinc in blast furnace ash samples is 0.23% - 0.87%, and the spiked recovery rate is 98% - 102%. However, this method is not applicable to the determination of the contents of potassium oxide and sodium oxide in blast furnace ash. Summary of the Invention

[0005] The present invention provides a method for detecting the contents of potassium oxide and sodium oxide in blast furnace ash, which has low cost, simple steps and easy operation, and realizes the detection of the contents of potassium oxide and sodium oxide in blast furnace ash.

[0006] In order to achieve the above object, the present invention is realized by adopting the following technical solutions: A method for detecting the contents of potassium oxide and sodium oxide in blast furnace ash, comprising the following steps: S1. Weigh 0.1 - 0.5 g of the blast furnace ash sample for production, roast it at high temperature to remove free carbon, and cool it to room temperature; S2. Moisten the sample with water, add 7 - 20 mL of concentrated hydrochloric acid, 5 - 10 mL of hydrofluoric acid, 5 - 10 mL of perchloric acid, and heat at 260 - 290 °C until perchloric acid fumes are evolved, and continue heating and evaporating until nearly dry; S3. Add 10 - 20 mL of hydrochloric acid, heat to dissolve the salts, transfer the solution into a plastic volumetric flask, cool to room temperature, dilute it with water to the set scale, and mix well to obtain the potassium and sodium standard solutions; S4. Take the potassium and sodium standard solutions and dilute them step by step to obtain a calibration curve, measure the calibration curve and the test solution with an atomic absorption spectrometer, and calculate the mass contents of potassium oxide and sodium oxide in the blast furnace ash: (1); Wherein, w is the mass content of potassium oxide or sodium oxide, w is w(K) or w(Na) ,w(K) is the mass content of potassium oxide in blast furnace ash, w(Na) is the mass content of sodium oxide in blast furnace ash; c is the content of potassium or sodium element obtained from the calibration curve, μg / mL; V is the fixed volume of the test solution to be measured, mL; m is the mass of the sample, g; Mass content of potassium oxide in blast furnace ash: w(K 2 O) = 1.2046× w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) = 1.3480× w(Na) (3).

[0007] Furthermore, the blast furnace ash sample for production is the blast furnace ash for production ground and mixed evenly to make a sample with a particle size less than 0.09 mm.

[0008] Furthermore, the high-temperature burning is to place the sample in a porcelain boat for high-temperature burning, and the burning temperature is 750 - 850 °C.

[0009] Furthermore, the step S2 is carried out in a polytetrafluoroethylene beaker.

[0010] Furthermore, in the step S2, the mass concentration of concentrated hydrochloric acid is 36 - 38%, the mass concentration of hydrofluoric acid is 40 - 41%, and the mass concentration of perchloric acid is 70 - 72%.

[0011] Furthermore, in the step S3, the hydrochloric acid is prepared by mixing concentrated hydrochloric acid and water at a volume ratio of 1:1 - 2.

[0012] Furthermore, the plastic volumetric flask is a 100 mL volumetric flask.

[0013] Furthermore, in the step S4, the potassium and sodium standard solutions are taken at 1000 μg / mL and diluted step by step to obtain the concentration range of the working curve: 0 μg / mL - 50 μg / mL.

[0014] Compared with the prior art, the beneficial effects of the present invention are: 1) The sample treatment cost of this method is low, the chemical reagents used are less, and the environmental impact is small; 2) Only basic laboratory equipment is required, which is suitable for most laboratories to adopt. The steps of treating samples are simple and easy to operate; 3) It realizes the detection of the contents of potassium oxide and sodium oxide in blast furnace ash, providing technical support for the smooth operation of the blast furnace. Specific embodiments

[0015] The following further describes the specific embodiments of the present invention: A method for detecting the contents of potassium oxide and sodium oxide in blast furnace ash according to the present invention includes the following steps: S1. Take the blast furnace ash for production, grind it finely and mix it evenly to make a sample with a particle size less than 0.09 mm. Weigh 0.1 - 0.5 g of the test sample, accurate to 0.0001 g. Place the test sample in a porcelain boat and burn it at a high temperature of 750 - 850 °C in a high-temperature furnace to remove free carbon completely, and then cool it to room temperature.

[0016] S2. Place the test sample in a polytetrafluoroethylene beaker, moisten the test sample with a small amount of water, add 7 - 20 mL of concentrated hydrochloric acid with a mass concentration of 36 - 38%, 5 - 10 mL of hydrofluoric acid with a mass concentration of 40%, 5 - 10 mL of perchloric acid with a mass concentration of 70 - 72%, and heat it at 260 - 290 °C until perchloric acid fumes are evolved. Continue to heat and evaporate until it is nearly dry, and then take it down.

[0017] S3. Add 10 - 20 mL of hydrochloric acid with a volume ratio of concentrated hydrochloric acid to water of 1:1 - 2, heat to dissolve salts, transfer the solution into a 100 mL plastic volumetric flask, cool to room temperature, dilute it to the mark with water, and mix evenly to obtain a potassium and sodium standard solution.

[0018] S4. Take a potassium and sodium standard solution of 1000 μg / mL, gradually dilute it to obtain a calibration curve. The concentration range of the working curve obtained by gradual dilution is: 0 μg / mL - 50 μg / mL. Use an atomic absorption spectrometer to measure the calibration curve and the test solution, and calculate the contents of potassium oxide and sodium oxide in the blast furnace ash using the following formula: (1); Wherein, w is the mass content of potassium oxide or sodium oxide, w is w(K) or w(Na) , w(K) is the mass content of potassium oxide in the blast furnace ash, w(Na) is the mass content of sodium oxide in the blast furnace ash; c is the content of potassium or sodium element obtained from the calibration curve, μg / mL; V is the constant volume of the test solution, mL; m is the mass of the test sample, g; Mass content of potassium oxide in blast furnace ash: w(K 2 O) = 1.2046× w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) = 1.3480× w(Na) (3).

[0019] The following embodiments are implemented on the premise of the technical solution of the present invention, and detailed implementation manners and specific operation processes are given. However, the protection scope of the present invention is not limited to the following embodiments. The methods used in the following embodiments are all conventional methods unless otherwise specified.

[0020] Example 1:

[0021] A method for detecting the contents of potassium oxide and sodium oxide in blast furnace ash of the present invention includes the following steps: S1. Take blast furnace ash 1# for production, grind it finely and mix it evenly to make a sample with a particle size less than 0.09 mm. Weigh 0.1 g of the test sample, accurate to 0.0001 g. Place the test sample in a porcelain boat and burn it at a high temperature of 750 °C in a high-temperature furnace to remove all free carbon and cool it to room temperature.

[0022] S2. Place the test sample in a polytetrafluoroethylene beaker, moisten the test sample with a small amount of water, add 7 mL of concentrated hydrochloric acid with a mass concentration of 36%, 5 mL of hydrofluoric acid with a mass concentration of 40%, and 5 mL of perchloric acid with a mass concentration of 70%. Heat it at 260 °C until perchloric acid fumes are evolved, and continue to heat and evaporate until nearly dry, then take it down.

[0023] S3. Add 10 mL of hydrochloric acid with a volume ratio of concentrated hydrochloric acid to water of 1:1, heat to dissolve the salts, transfer the solution into a 100 mL plastic volumetric flask, cool to room temperature, dilute it to the mark with water, and mix well to obtain a potassium and sodium standard solution.

[0024] S4. Take a potassium and sodium standard solution of 1000 μg / mL and gradually dilute it to obtain a calibration curve. The concentration range is: 0 μg / mL, 1 μg / mL, 3 μg / mL, 5 μg / mL, 7 μg / mL, 10 μg / mL. Use an atomic absorption spectrometer to measure the calibration curve and the test solution, and calculate the contents of potassium oxide and sodium oxide in the blast furnace ash using the following formula: (1); Wherein, w is the mass content of potassium oxide or sodium oxide, w is w(K) or w(Na) , w(K) is the mass content of potassium oxide in the blast furnace ash, w(Na) is the mass content of sodium oxide in the blast furnace ash; c is the content of potassium or sodium element obtained from the calibration curve, μg / mL; V is the constant volume of the test solution, mL; m is the mass of the test sample, g; The atomic weight of potassium is 39.0983 g / mol, the atomic weight of sodium is 22.9898 g / mol, and the atomic weight of oxygen is 15.9994 g / mol. The molecular weight of potassium oxide is 94.1960 g / mol, and the molecular weight of sodium oxide is 61.9790 g / mol. After calculation, the conversion contents of potassium oxide and sodium oxide are obtained: Mass content of potassium oxide in blast furnace ash: w(K 2 O) = 1.2046 × w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) = 1.3480 × w(Na) (3); The potassium oxide content measured by this method in the blast furnace ash of No. 1 is 0.62%, and the sodium oxide content is 0.43%.

[0025] Example 2:

[0026] A method for detecting the contents of potassium oxide and sodium oxide in blast furnace ash according to the present invention includes the following steps: S1. Take the blast furnace ash No. 2 for production, grind it finely and mix it evenly to make a sample with a particle size less than 0.09 mm. Weigh 0.2 g of the sample, accurate to 0.0001 g. Place the sample in a porcelain boat and burn it at a high temperature of 800 °C in a high-temperature furnace to remove free carbon and cool it to room temperature.

[0027] S2. Place the sample in a polytetrafluoroethylene beaker, moisten the sample with a small amount of water, add 10 mL of concentrated hydrochloric acid with a mass concentration of 37%, 7 mL of hydrofluoric acid with a mass concentration of 40%, and 7 mL of perchloric acid with a mass concentration of 71%. Heat it at 270 °C until perchloric acid fumes are emitted, and continue to heat and evaporate until it is nearly dry, then take it down.

[0028] S3. Add 10 mL of hydrochloric acid with a volume ratio of concentrated hydrochloric acid to water of 1:2, heat to dissolve the salts, transfer the solution into a 100 mL plastic volumetric flask, cool to room temperature, dilute it to the mark with water, and mix evenly to obtain a potassium and sodium standard solution.

[0029] S4. Take the potassium and sodium standard solution of 1000 μg / mL and dilute it step by step to obtain a calibration curve with a concentration range of: 0 μg / mL, 1 μg / mL, 5 μg / mL, 510 μg / mL, 15 μg / mL, 20 μg / mL. Use an atomic absorption spectrometer to measure the calibration curve and the solution to be measured, and calculate the contents of potassium oxide and sodium oxide in the blast furnace ash with the following formula: (1); Wherein, w is the mass content of potassium oxide or sodium oxide, w isw(K) or w(Na) , w(K) is the mass content of potassium oxide in blast furnace ash, w(Na) is the mass content of sodium oxide in blast furnace ash; c is the content of potassium or sodium element obtained from the calibration curve, μg / mL; V is the fixed volume of the solution to be measured, mL; m is the mass of the sample, g; The atomic weight of potassium element is 39.0983 g / mol, the atomic weight of sodium element is 22.9898 g / mol, the atomic weight of oxygen element is 15.9994 g / mol, the molecular weight of potassium oxide is 94.1960 g / mol, and the molecular weight of sodium oxide is 61.9790 g / mol. After calculation, the conversion contents of potassium oxide and sodium oxide are obtained: Mass content of potassium oxide in blast furnace ash: w(K 2 O) = 1.2046× w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) = 1.3480× w(Na) (3); The potassium oxide content of the 2# blast furnace ash measured by this method is 0.47%, and the sodium oxide content is 0.38%.

[0030] Example 3:

[0031] A method for detecting the contents of potassium oxide and sodium oxide in blast furnace ash according to the present invention includes the following steps: S1. Take the 3# blast furnace ash for production, grind and mix it evenly to make a sample with a particle size less than 0.09 mm. Weigh 0.3 g of the sample, accurate to 0.0001 g. Place the sample in a porcelain boat and burn it at 800 °C in a high-temperature furnace to remove free carbon completely, and then cool it to room temperature.

[0032] S2. Place the sample in a polytetrafluoroethylene beaker, moisten the sample with a small amount of water, add 12 mL of concentrated hydrochloric acid with a mass concentration of 38%, 7 mL of hydrofluoric acid with a mass concentration of 40%, and 7 mL of perchloric acid with a mass concentration of 72%. Heat it at 280 °C until perchloric acid fumes are emitted, and continue to heat and evaporate until it is nearly dry, then take it down.

[0033] S3. Add 15 mL of hydrochloric acid with a volume ratio of concentrated hydrochloric acid to water of 1:2, heat to dissolve the salts, transfer the solution into a 100 mL plastic volumetric flask, cool it to room temperature, dilute it to the mark with water, and mix well to obtain a potassium and sodium standard solution.

[0034] S4. Take 1000 μg / mL potassium and sodium standard solutions, and gradually dilute them to obtain a calibration curve with a concentration range of: 0 μg / mL, 5 μg / mL, 10 μg / mL, 15 μg / mL, 20 μg / mL, 30 μg / mL. Use an atomic absorption spectrometer to measure the calibration curve and the solution to be measured, and calculate the potassium oxide and sodium oxide contents in blast furnace ash using the following formula: (1); Wherein, w is the mass content of potassium oxide or sodium oxide, w is w(K) or w(Na) , w(K) is the mass content of potassium oxide in blast furnace ash, w(Na) is the mass content of sodium oxide in blast furnace ash; c is the content of potassium or sodium element obtained from the calibration curve, μg / mL; V is the fixed volume of the solution to be measured, mL; m is the mass of the sample, g; The atomic weight of potassium element is 39.0983 g / mol, the atomic weight of sodium element is 22.9898 g / mol, the atomic weight of oxygen element is 15.9994 g / mol. The molecular weight of potassium oxide is 94.1960 g / mol, and the molecular weight of sodium oxide is 61.9790 g / mol. After calculation, the conversion contents of potassium oxide and sodium oxide are obtained: Mass content of potassium oxide in blast furnace ash: w(K 2 O) = 1.2046× w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) = 1.3480× w(Na) (3); The potassium oxide content of the 3# blast furnace ash measured by this method is 0.65%, and the sodium oxide content is 0.48%.

[0035] Example 4:

[0036] A method for detecting the potassium oxide and sodium oxide contents in blast furnace ash according to the present invention includes the following steps: S1. Take the 4# blast furnace ash for production, grind it finely and mix it evenly to make a sample with a particle size less than 0.09 mm. Weigh 0.4 g of the sample, accurate to 0.0001 g. Place the sample in a porcelain boat and burn it at 850 °C in a high-temperature furnace to remove free carbon, and then cool it to room temperature.

[0037] S2. Place the sample in a polytetrafluoroethylene beaker, moisten the sample with a small amount of water, add 15 mL of concentrated hydrochloric acid with a mass concentration of 38%, 10 mL of hydrofluoric acid with a mass concentration of 40%, 10 mL of perchloric acid with a mass concentration of 72%, heat at 290 °C until perchloric acid fumes are evolved, continue heating and evaporating until nearly dry, and then remove from the heat.

[0038] S3. Add 20 mL of hydrochloric acid with a volume ratio of concentrated hydrochloric acid to water of 1:1, heat to dissolve the salts, transfer the solution to a 100 mL plastic volumetric flask, cool to room temperature, dilute to the mark with water, and mix well to obtain a potassium and sodium standard solution.

[0039] S4. Take the potassium and sodium standard solution of 1000 μg / mL and dilute it step by step to obtain a calibration curve with a concentration range of: 0 μg / mL, 5 μg / mL, 10 μg / mL, 20 μg / mL, 30 μg / mL, 40 μg / mL. Use an atomic absorption spectrometer to measure the calibration curve and the solution to be measured, and calculate the contents of potassium oxide and sodium oxide in the blast furnace ash using the following formula: (1); Wherein, w is the mass content of potassium oxide or sodium oxide, w is w(K) or w(Na) , w(K) is the mass content of potassium oxide in the blast furnace ash, w(Na) is the mass content of sodium oxide in the blast furnace ash; c is the content of potassium or sodium element obtained from the calibration curve, μg / mL; V is the constant volume of the solution to be measured, mL; m is the mass of the sample, g; The atomic weight of potassium element is 39.0983 g / mol, the atomic weight of sodium element is 22.9898 g / mol, the atomic weight of oxygen element is 15.9994 g / mol, the molecular weight of potassium oxide is 94.1960 g / mol, and the molecular weight of sodium oxide is 61.9790 g / mol. After calculation, the conversion contents of potassium oxide and sodium oxide are obtained: Mass content of potassium oxide in blast furnace ash: w(K 2 O) = 1.2046× w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) = 1.3480× w(Na) (3); The potassium oxide content of the No. 4 blast furnace ash measured by this method is 0.49%, and the sodium oxide content is 0.31%.

[0040] Example 5:

[0041] A method for detecting the potassium oxide and sodium oxide content in blast furnace ash according to the present invention comprises the following steps: S1. Take 5# blast furnace ash for production, grind it finely and mix it evenly to make a sample with a particle size less than 0.09 mm. Weigh 0.5 g of the test sample accurately to 0.0001 g. Place the test sample in a porcelain boat and burn it at 800 °C in a high-temperature furnace to remove free carbon completely, and then cool it to room temperature.

[0042] S2. Place the test sample in a polytetrafluoroethylene beaker, moisten the test sample with a small amount of water, add 20 mL of concentrated hydrochloric acid with a mass concentration of 36 - 38%, 10 mL of hydrofluoric acid with a mass concentration of 40%, and 10 mL of perchloric acid with a mass concentration of 71%. Heat it at 280 °C until perchloric acid fumes are evolved, and continue heating and evaporating until it is nearly dry, then take it down.

[0043] S3. Add 20 mL of hydrochloric acid with a volume ratio of concentrated hydrochloric acid to water of 1:1, heat to dissolve salts, transfer the solution into a 100 mL plastic volumetric flask, cool to room temperature, dilute it to the scale with water, and mix evenly to obtain a potassium and sodium standard solution.

[0044] S4. Take a potassium and sodium standard solution of 1000 μg / mL and dilute it step by step to obtain a calibration curve with a concentration range of: 0 μg / mL, 10 μg / mL, 20 μg / mL, 30 μg / mL, 40 μg / mL, 50 μg / mL. Measure the calibration curve and the test solution with an atomic absorption spectrometer, and calculate the potassium oxide and sodium oxide content in the blast furnace ash using the following formula: (1); Wherein, w is the mass content of potassium oxide or sodium oxide, w is w(K) or w(Na) , w(K) is the mass content of potassium oxide in the blast furnace ash, w(Na) is the mass content of sodium oxide in the blast furnace ash; c is the content of potassium or sodium element obtained from the calibration curve, μg / mL; V is the constant volume of the test solution, mL; m is the mass of the test sample, g; The atomic weight of potassium element is 39.0983 g / mol, the atomic weight of sodium element is 22.9898 g / mol, the atomic weight of oxygen element is 15.9994 g / mol, the molecular weight of potassium oxide is 94.1960 g / mol, and the molecular weight of sodium oxide is 61.9790 g / mol. After calculation, the conversion content of potassium oxide and sodium oxide is obtained: The mass content of potassium oxide in the blast furnace ash: w(K 2 O) = 1.2046 ×w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) = 1.3480 × w(Na) (3); The potassium oxide content of the blast furnace ash of No. 4 measured by this method is 0.73%, and the sodium oxide content is 0.28%.

Claims

1. A method for detecting the content of potassium oxide and sodium oxide in blast furnace ash, characterized in that: The steps include: S1. Weigh 0.1-0.5g of blast furnace ash sample for production, burn it at high temperature to remove free carbon, and cool it to room temperature; S2. Wet the sample with water, add 7-20 mL of concentrated hydrochloric acid, 5-10 mL of hydrofluoric acid, and 5-10 mL of perchloric acid, heat at 260-290°C until perchloric acid smoke appears, and continue heating and evaporating until nearly dry; S3, add 10-20 mL of hydrochloric acid, heat to dissolve the salts, transfer the solution into a plastic volumetric flask, cool to room temperature, dilute with water to the set scale, and mix to obtain potassium and sodium standard solutions; S4. Take potassium and sodium standard solutions and dilute them step by step to obtain a calibration curve. Use an atomic absorption spectrometer to measure the calibration curve and the solution to be tested, and calculate the mass content of potassium oxide and sodium oxide in blast furnace ash: (1); in, w is the mass content of potassium oxide or sodium oxide, w for w(K) or w(Na) , w(K) is the mass content of potassium oxide in blast furnace ash, w(Na) is the mass content of sodium oxide in blast furnace ash; c is the potassium or sodium content obtained from the calibration curve, μg / mL; V is the volume of the solution to be tested, mL; m is the mass of the sample, g; Mass content of potassium oxide in blast furnace ash: w(K 2 O) =1.2046× w(K) (2); Mass content of sodium oxide in blast furnace ash: w(Na 2 O) =1.3480× w(Na) (3).

2. The method for detecting the content of potassium oxide and sodium oxide in blast furnace ash according to claim 1, characterized in that: The production blast furnace ash sample is obtained by grinding and mixing the production blast furnace ash to make a sample with a particle size less than 0.09 mm.

3. The method for detecting the content of potassium oxide and sodium oxide in blast furnace ash according to claim 1, characterized in that: The high temperature calcination is to place the sample in a porcelain boat and calcine it at a high temperature, and the calcination temperature is 750-850°C.

4. The method for detecting the content of potassium oxide and sodium oxide in blast furnace ash according to claim 1, characterized in that: The step S2 is performed in a polytetrafluoroethylene beaker.

5. The method for detecting the content of potassium oxide and sodium oxide in blast furnace ash according to claim 1, characterized in that: In step S2, the mass concentration of concentrated hydrochloric acid is 36-38%, the mass concentration of hydrofluoric acid is 40-41%, and the mass concentration of perchloric acid is 70-72%.

6. The method for detecting the content of potassium oxide and sodium oxide in blast furnace ash according to claim 1, characterized in that: In step S3, the hydrochloric acid is prepared by mixing concentrated hydrochloric acid with water in a volume ratio of 1:1 to 2.

7. The method for detecting the content of potassium oxide and sodium oxide in blast furnace ash according to claim 1, characterized in that: The plastic volumetric flask is a 100 mL volumetric flask.

8. The method for detecting the content of potassium oxide and sodium oxide in blast furnace ash according to claim 1, characterized in that: In step S4, the potassium and sodium standard solutions are taken at 1000 μg / mL, and are diluted step by step to obtain a concentration range of the working curve: 0 μg / mL to 50 μg / mL.

Citation Information

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